[Code of Federal Regulations] [Title 21, Volume 3] [Revised as of April 1, 2001] From the U.S. Government Printing Office via GPO Access [CITE: 21CFR177.1330] [Page 247-250] TITLE 21--FOOD AND DRUGS CHAPTER I--FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) PART 177--INDIRECT FOOD ADDITIVES: POLYMERS--Table of Contents Subpart B--Substances for Use as Basic Components of Single and Repeated Use Food Contact Surfaces Sec. 177.1330 Ionomeric resins. Ionomeric resins manufactured from either ethylene-methacrylic acid copolymers (and/or their ammonium, calcium, magnesium, potassium, sodium, and/or zinc partial salts), ethylene-methacrylic acid-vinyl acetate copolymers (and/or their ammonium, calcium, magnesium, potassium, sodium, and/or zinc partial salts,), or methacrylic acid polymers with ethylene and isobutyl acrylate (and/or their potassium, sodium and/or zinc partial salts) may be safely used as articles or components of articles intended for use in contact with food, in accordance with the following prescribed conditions: (a) For the purpose of this section, the ethylene-methacrylic acid copolymers consist of basic copolymers produced by the copolymerization of ethylene and methacrylic acid such that the copolymers contain no more than 20 weight percent of polymer units derived from methacrylic acid, and the ethylene-methacrylic acid-vinyl acetate copolymers consist of basic copolymers produced by the copolymerization of ethylene, methacrylic acid, and vinyl acetate such that the copolymers contain no more than 15 weight percent of polymer units derived from methacrylic acid. (b) For the purpose of this section, the methacrylic acid copolymers with ethylene and isobutyl acrylate consist of basic copolymers produced by the copolymerization of methacrylic acid, ethylene, and isobutyl acrylate such that the copolymers contain no less than 70 weight percent of polymer units derived from ethylene, no more than 15 weight percent of polymer units derived from methacrylic acid, and no more than 20 weight percent of polymer units derived from isobutyl acrylate. From 20 percent to 70 percent of the carboxylic acid groups may optionally be neutralized to form sodium or zinc salts. (c) The finished food-contact article described in paragraph (a) of this section, when extracted with the solvent or solvents characterizing the type of food and under the conditions of time and temperature characterizing the conditions of its intended use as determined from tables 1 and 2 of Sec. 176.170(c) [[Page 248]] of this chapter, yields net acidified chloroform-soluble extractives in each extracting solvent not to exceed 0.5 milligram per square inch of food-contact surface when tested by the methods described in paragraph (e)(1) of this section, and if the finished food-contact article is itself the subject of a regulation in parts 174, 175, 176, 177, 178 and Sec. 179.45 of this chapter, it shall also comply with any specifications and limitations prescribed for it by that regulation. Note: In testing the finished food-contact article, use a separate test sample for each required extracting solvent. (d) The finished food-contact article described in paragraph (b) of this section, when extracted according to the methods listed in paragraph (e)(2) of this section and referenced in this paragraph (d), using the solvent or solvents characterizing the type of food as determined from table I of paragraph (f) of this section, shall yield net acidified chloroform-soluble extractives as follows: (1) For fatty food use. (i) For films of 2 mil (0.002 inches) thickness or less, extractives shall not exceed 0.70 milligram/square inch \1\ (0.109 milligram/square centimeter) of food-contact surface (n- heptane extractions) when extracted by the abbreviated method cited in paragraph (e)(2)(i) of this section. --------------------------------------------------------------------------- \1\ Average of four separate values, no single value of which differs from the average of those values by more then plus-minus10 percent. --------------------------------------------------------------------------- (ii) For films of greater than 2 mils (0.002 inch) thickness, extractives shall not exceed 0.40 milligram/square inch 1 (0.062 milligram/square centimeter) of food-contact surface (n-heptane extractions) when extracted by the abbreviated method cited in paragraph (e)(2)(i) of this section, or (iii) Alternatively, for films of greater than 2 mils thickness, extractives shall not exceed 0.70 milligram/square inch \1\ (0.109 milligram/square centimeter) of food-contact surface (n-heptane extractions) when extracted by the equilibrium method cited in paragraph (e)(2)(ii) of this section. (2) For aqueous foods. (i) The net acidified chloroform-soluble extractives shall not exceed 0.02 milligram/square inch \2\(0.003 milligram/square centimeter) of food-contact surface (water, acetic acid, or ethanol/water extractions) when extracted by the abbreviated method cited in paragraph (e)(2)(i) of this section. --------------------------------------------------------------------------- \2\ Average of four separate values, no single value of which differs from the average of those values by more than plus-minus50 percent. --------------------------------------------------------------------------- (ii) Alternatively, the net acidified chloroform-soluble extractives shall not exceed 0.05 milligram/square inch \3\ (0.078 mg/square centimeter) of food-contact surface (water, acetic acid, or ethanol/ water extractions) when extracted by the equilibrium method cited in paragraph (e)(2)(ii) of this section. If when exposed to n-heptane, a particular film splits along die lines, thus permitting exposure of both sides of the film to the extracting solvent, the results for that film sample are invalid and the test must be repeated for that sample until no splitting by the solvent occurs. If the finished food-contact article is itself the subject of a regulation in parts 174, 175, 176, 177, 178 and Sec. 179.45 of this chapter, it shall also comply with any specifications and limitations prescribed for it by that regulation. --------------------------------------------------------------------------- \3\See footnote 2 to paragraph (d)(2)(i) of this section. --------------------------------------------------------------------------- Note: In testing the finished food-contact article, use a separate test sample for each required extracting solvent. (e) Analytical methods--(1) Selection of extractability conditions for ionomeric resins. First ascertain the type of food (table 1 of Sec. 176.170(c) of this chapter) that is being packed or used in contact with the finished food-contact article described in paragraph (a) of this section, and also ascertain the normal conditions of thermal treatment used in packaging or contacting the type of food involved. Using table 2 of Sec. 176.170 (c) of this chapter, select the food- simulating solvent or solvents and the time-temperature test conditions that correspond to the intended use of the finished food-contact article. Having selected the appropriate food-simulating solvent or solvents and time-temperature exaggeration over normal use, follow the applicable extraction procedure. (2) Selection of extractability conditions for ionomeric resins. Using table I of [[Page 249]] paragraph (f) of this section ascertain the type of food that is being packed or used in contact with the finished food-contact article described in paragraph (b) of this section, and also ascertain the food- simulating solvent or solvents that correspond to the intended use of the finished food-contact article. (i) Abbreviated test. For intended use involving food contact at or below 120 deg.F (49 deg.C), the appropriate food-simulating solvent is to contact the food-contact film for the time and temperatures as follows: ------------------------------------------------------------------------ Solvent Time Temperature ------------------------------------------------------------------------ n-Heptane............................ \1\ 2 120 deg.F (49 deg.C). Water, 3% acetic acid, or 8%/50% \1\ 48 120 deg.F (49 deg.C). ethanol. ------------------------------------------------------------------------ \1\ Hours (ii) Equilibrium test. For intended use involving food contact at or below 120 deg.F (49 deg.C), the appropriate food-simulating solvent is to contact the food-contact film at a temperature of 120 deg.F until equilibrium is demonstrated. ------------------------------------------------------------------------ Minimum extraction Solvent times (hours) ------------------------------------------------------------------------ n-Heptane................................................... 8, 10, 12 Water, 3% acetic acid, or 8%/50% ethanol.................... 72, 96, 120 ------------------------------------------------------------------------ The results from a series of extraction times demonstrate equilibrium when the net chloroform-soluble extractives are unchanging within experimental error appropriate to the method as described in paragraphs (d) (1)(i) and (2)(i) of this section. Should equilibrium not be demonstrated over the above time series, extraction times must be extended until three successive unchanging values for extractives are obtained. In the case where intended uses involve temporary food contact above 120 deg.F, the food-simulating solvent is to be contacted with the food-contact article under conditions of time and temperature that duplicate the actual conditions in the intended use. Subsequently the extraction is to be continued for the time period and under the conditions specified in the above table. (3) Reagents--(i) Water. All water used in extraction procedures should be freshly demineralized (deionized) distilled water. (ii) n-Heptane. Reagent grade, freshly redistilled before use, using only material boiling at 208 deg.F (97.8 deg.C). (iii) Alcohol. 8 or 50 percent (by volume), prepared from undenatured 95 percent ethyl alcohol diluted with demineralized (deionized), distilled water. (iv) Chloroform. Reagent grade, freshly redistilled before use, or a grade having an established, consistently low blank. (v) Acetic acid. 3 percent (by weight), prepared from glacial acetic acid diluted with demineralized (deionized), distilled water. (4) Selection of test method. The finished food-contact articles shall be tested either by the extraction cell described in the Journal of the Association of Official Agricultural Chemists, Vol. 47, No. 1, p. 177-179 (February 1964), also described in ASTM method F34-76 (Reapproved 1980), ``Standard Test Method for Liquid Extraction of Flexible Barrier Materials,'' which are incorporated by reference, or by adapting the in-container methods described in Sec. 175.300(e) of this chapter. Copies of the material incorporated by reference are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 200 C St. SW., Washington, DC 20204, and the American Society for Testing Materials, 1916 Race St., Philadelphia, PA 19103, respectively, or may be examined at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC 20408. (5) Selection of samples. Quadruplicate samples should be tested, using for each replicate sample the number of finished articles with a food-contact surface nearest to 100 square inches. (6) Determination of amount of extractives--(i) Total residues. At the end of the exposure period, remove the test container or test cell from the oven, if any, and combine the solvent for each replicate in a clean Pyrex (or equivalent) flask or beaker, being sure to rinse the test container or cell with a small quantity of clean solvent. Evaporate the food-simulating solvents to about 100 milliliters in the flask, and transfer to a clean, tared evaporating dish (platinum or Pyrex), washing the flask three times with small portions [[Page 250]] of solvent used in the extraction procedure, and evaporate to a few milliliters on a nonsparking, low-temperature hotplate. The last few milliliters should be evaporated in an oven maintained at a temperature of 221 deg.F (105 deg.C). Cool the evaporating dish in a desiccator for 30 minutes and weigh the residues to the nearest 0.1 milligram, e. Calculate the extractives in milligrams per square inch of the container or material surface. (a) Water, 3 percent acetic acid, and 8 percent and 50 percent alcohol. Milligrams extractives per square inch=e/s. (b) Heptane. Milligrams extractives per square inch=(e)/(s)(F) where: e=Milligrams extractives per sample tested. s=Surface area tested, in square inches. F=Five, the ratio of the amount of extractives removed by heptane under exaggerated time-temperature test conditions compared to the amount extracted by a fat or oil under exaggerated conditions of thermal sterilization and use. e'=Acidified chloroform-soluble extractives residue. e' is substituted for e in the above equations when necessary (See paragraph (e)(6)(ii) of this section for method to obtain e'). If when calculated by the equations in paragraphs (e)(6)(i) (a) and (b) of this section, the extractives in milligrams per square inch exceed the limitations prescribed in paragraphs (c) or (d) of this section, proceed to paragraph (e)(6)(ii) of this section (method for determining the amount of acidified chloroform-soluble extractives residue). (ii) Acidified chloroform-soluble extractives residue. Add 3 milliliters of 37 percent ACS reagent grade hydrochloric acid and 3 milliliters of distilled water to the evaporating dish containing the dried and weighed residue, e, obtained in paragraph (e)(6)(i) of this section. Mix well so every portion of the residue is wetted with the hydrochloric acid solution. Then add 50 milliliters of chloroform. Warm carefully, and filter through Whatman No. 41 filter paper (or equivalent) in a Pyrex (or equivalent) funnel, collecting the filtrate in a clean separatory funnel. Shake for 1 minute, then draw off the chloroform layer into a clean tared evaporating dish (platinum or Pyrex). Repeat the chloroform extraction, washing the dish, the filter paper, and the separatory funnel with this second portion of chloroform. Add this filtrate to the original filtrate and evaporate the total down to a few milliliters on a low-temperature hotplate. The last few milliliters should be evaporated in an oven maintained at 221 deg.F. Cool the evaporating dish in a desiccator for 30 minutes and weigh to the nearest 0.1 milligram to get the acidified chloroform-soluble extractives residue, e'. This e' is substituted for e in the equations in paragraphs (e)(6)(i) (a) and (b) of this section. (f) The types of food and appropriate solvents are as follows: Table 1 ------------------------------------------------------------------------ Types of food Appropriate solvent ------------------------------------------------------------------------ 1. Nonacid (pH above 5.0), aqueous Water, n-heptane. products; may contain salt or sugar or both, and including oil-in-water emulsions of low- or high-fat content. 2. Acidic (pH 5.0 or below), aqueous n-heptane, water, 3% acetic products; may contain salt or sugar acid. or both, and including oil-in-water emulsions of low- or high-fat content. 3. Aqueous, acid or nonacid products Water, n-heptane, 3% acetic containing free oil or fat; may acid. contain salt, and including water-in- oil emulsions of low- or high-fat content. 4. Dairy products and modifications: Water, n-heptane.................... i. Water-in-oil emulsions, high or low fat. ii. Oil-in-water emulsions, high or low fat. 5. Low moisture fats and oils......... n-heptane. 6. Beverages: i. Containing up to 8% alcohol...... 8% ethanol/water. ii. Nonalcoholic.................... 3% acetic acid. iii. Containing more than 8% alcohol 50% ethanol/water. 7. Bakery products.................... Water, n-heptane. 8. Dry solids (without free fat or No extraction test required. oil). 9. Dry solids (with free fat or oil).. n-heptane. ------------------------------------------------------------------------ (g) The provisions of paragraphs (c) and (d) of this section are not applicable to the ionomeric resins that are used in food-packaging adhesives complying with Sec. 175.105 of this chapter. [45 FR 22916, Apr. 4, 1980, as amended at 49 FR 10108, Mar. 19, 1984; 49 FR 37747, Sept. 26, 1984; 53 FR 44009, Nov. 1, 1988; 54 FR 24898, June 12, 1989] [[Page 251]]